WO2017043117A1 - Oxyfluorure d'yttrium, poudre de matériau de départ pour la production d'oxyfluorure d'yttrium stabilisé, et procédé de production d'oxyfluorure d'yttrium stabilisé - Google Patents

Oxyfluorure d'yttrium, poudre de matériau de départ pour la production d'oxyfluorure d'yttrium stabilisé, et procédé de production d'oxyfluorure d'yttrium stabilisé Download PDF

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WO2017043117A1
WO2017043117A1 PCT/JP2016/060240 JP2016060240W WO2017043117A1 WO 2017043117 A1 WO2017043117 A1 WO 2017043117A1 JP 2016060240 W JP2016060240 W JP 2016060240W WO 2017043117 A1 WO2017043117 A1 WO 2017043117A1
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powder
yttrium oxyfluoride
yttrium
represented
oxyfluoride
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PCT/JP2016/060240
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Japanese (ja)
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康博 瀬戸
祥治 今浦
将大 小出
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三井金属鉱業株式会社
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Priority to KR1020187003031A priority Critical patent/KR101861983B1/ko
Priority to CN201680045497.6A priority patent/CN107848831A/zh
Priority to US15/749,432 priority patent/US10280091B2/en
Priority to JP2017502743A priority patent/JP6189570B2/ja
Publication of WO2017043117A1 publication Critical patent/WO2017043117A1/fr

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Definitions

  • the present invention relates to yttrium oxyfluoride having a cubic crystal structure stabilized by using a specific compound, a raw material powder for producing the stabilized yttrium oxyfluoride, and a method for producing the stabilized yttrium oxyfluoride.
  • Yttrium oxyfluoride has been used in various applications such as phosphorescent materials for ink production and molds for casting high melting point reactive metals (Patent Documents 1 and 2). Moreover, it has been reported that yttrium oxyfluoride has a high resistance to halogen-based plasma of a sprayed coating obtained when this is used as a spraying material (Patent Document 3).
  • Yttrium oxyfluoride represented by YOF usually has a rhombohedral crystal structure at room temperature, a cubic or tetragonal crystal structure at a temperature higher than 600 ° C., and 550 to 600 ° C. when cooled from a high temperature. It is known to exhibit a phase transition from cubic or tetragonal to rhombohedral. Since this phase transition is accompanied by a volume change, stress associated with the phase transition is generated during cooling in yttrium oxyfluoride. When yttrium oxyfluoride is heated from room temperature to a temperature higher than 600 ° C., stress due to the same phase transition is generated. For example, if yttrium oxyfluoride has a shape that is greatly affected by distortion due to volume change, such as a film or a bulk, this stress causes cracks and cracks.
  • An object of the present invention is to provide yttrium oxyfluoride that can eliminate various drawbacks of the above-described conventional technology.
  • the present invention is based on the above findings and provides yttrium oxyfluoride represented by YOF that is stabilized by calcium fluoride represented by CaF 2 .
  • the present invention also provides a raw material powder for producing stabilized yttrium oxyfluoride, comprising a mixed powder containing calcium fluoride powder represented by CaF 2 and yttrium oxyfluoride powder represented by YOF.
  • the present invention is a stable powder comprising a mixed powder containing calcium fluoride powder represented by CaF 2 , yttrium fluoride powder represented by YF 3 , and yttrium oxide powder represented by Y 2 O 3.
  • a raw material powder for producing yttrium oxyfluoride is provided.
  • the present invention provides a molded product of a mixed powder containing calcium fluoride powder represented by CaF 2 and yttrium oxyfluoride powder represented by YOF, in an inert atmosphere or under vacuum, at 800 ° C. or higher and 1700 ° C.
  • the manufacturing method of the stabilized yttrium oxyfluoride including the process of baking below is provided.
  • the present invention provides a compact of a mixed powder containing calcium fluoride powder represented by CaF 2 , yttrium fluoride powder represented by YF 3 , and yttrium oxide powder represented by Y 2 O 3. Firing to produce yttrium oxyfluoride represented by YOF from YF 3 and Y 2 O 3 , and then firing at 800 ° C. to 1700 ° C. in an inert atmosphere or under vacuum. A method for producing yttrium fluoride is provided.
  • the phase transition between cubic or tetragonal crystals and rhombohedral crystals during heating or cooling is effectively prevented.
  • the yttrium oxyfluoride of the present invention can effectively prevent cracking and cracking during heating or cooling in the case of using a sintered body or a sprayed film.
  • the said yttrium oxyfluoride can be suitably manufactured by using the raw material powder for manufacturing the stabilized yttrium oxyfluoride of this invention.
  • the above-described yttrium oxyfluoride can be suitably produced by the method for producing stabilized yttrium oxyfluoride of the present invention.
  • DTA differential thermal analysis
  • TMA thermomechanical analysis
  • X: Y is a compound in which X is 0.9 to 1.1 and Y is 0.9 to 1.1.
  • X or Y is 1, more preferably X and Y are 1.
  • One of the characteristics of the yttrium oxyfluoride of the present invention is that it is stabilized using a fluoride represented by CaF 2 as a stabilizer.
  • stabilized yttrium oxyfluoride means that the cubic state of yttrium oxyfluoride in a low-temperature phase of less than 550 ° C. is stabilized as compared with a pure yttrium oxyfluoride product.
  • yttrium oxyfluoride of the present invention stabilized by CaF 2 has a cubic crystal phase at 25 ° C.
  • the fact that yttrium oxyfluoride is stabilized may be confirmed by any one of the following three methods, for example.
  • the determination is centered on whether or not a specific rhombohedral peak exists.
  • the above-mentioned specific peak intensity in the rhombohedral crystal is not observed, or the specific peak satisfies the specific condition on the premise that no XRD peak due to YOF other than cubic and rhombohedral is observed.
  • yttrium oxyfluoride When observed very small, it can be said that yttrium oxyfluoride is stabilized.
  • the ratio of peak intensity here is measured as a ratio of peak height.
  • the YOF peak position and the peak reflection surface index by XRD measurement are based on the description of the ICDD card.
  • a method of subjecting yttrium oxyfluoride to DTA measurement at a heating rate of 5 ° C./min from 25 ° C. to 1000 ° C. can be mentioned.
  • the yttrium oxyfluoride is stabilized when no endothermic peak derived from the phase transition from cubic or tetragonal to rhombohedral is observed in the range of 550 to 600 ° C.
  • the DTA measurement can be performed by the method described in Examples described later.
  • yttrium oxyfluoride is subjected to TMA measurement at a temperature decrease rate of 5 ° C./min from 1000 ° C. to 25 ° C.
  • the term “having discontinuous points of dimensional change” in the present invention means that two bending points are recognized at the time of temperature rise or at the time of temperature fall in TMA measurement. More specifically, the judgment is as follows. For example, in the TMA measurement of Comparative Example 1 in FIG.
  • the TMA curve has a discontinuous point when the low temperature side of these two bending points is T1 and the high temperature side is T2, for example, the tangent line of the TMA curve at the point 10 ° C. away from the low temperature side and T1 And the tangent line of the TMA curve located at the center of T2 do not intersect other than one intersection and do not have the same inclination.
  • the TMA measurement can be performed by the method described in Examples described later.
  • the yttrium oxyfluoride of the present invention is stabilized by any one of the three methods mentioned above, it is defined that the yttrium oxyfluoride is stabilized.
  • the yttrium oxyfluoride of the present invention is preferably a solid solution in which a fluoride represented by CaF 2 is dissolved in yttrium oxyfluoride represented by YOF.
  • the peak derived from the fluoride represented by CaF 2 is not observed.
  • the presence of the elements Ca and fluorine can be confirmed by a fluorescent X-ray analysis method or the like.
  • the powder X-ray diffraction measurement is performed by the method described in the examples described later.
  • a peak derived from a fluoride represented by CaF 2 is not observed in the powder X-ray diffraction measurement of the scanning range and the radiation source.
  • a part of the fluoride may be present in a form not dissolved in yttrium oxyfluoride.
  • a peak derived from a fluoride represented by CaF 2 may be observed within a range where the effects of the present invention are not impaired.
  • the number of moles of Ca is preferably 10 to 40 moles relative to 100 moles of yttrium (Y).
  • Y yttrium
  • the number of moles of Ca with respect to the number of moles of yttrium (Y) is 40 moles or less, the amount of fluoride represented by CaF 2 that precipitates without dissolving in yttrium oxyfluoride can be suppressed.
  • the influence of the presence of fluoride on the physical properties of yttrium oxyfluoride can be suppressed.
  • the ratio of the number of moles of Ca to the number of moles of 100 moles of yttrium (Y) is more preferably 15 to 35 moles, and particularly preferably 15 to 30 moles. It is particularly preferable that the amount be 15 mol or more and 25 mol or less.
  • the number of moles of yttrium (Y) and the number of moles of Ca in yttrium oxyfluoride can be measured by the following method. That is, it can be measured by calculating the molar concentration from the results of quantitative analysis of Ca and Y by an analytical method such as a fluorescent X-ray method, ICP-AES method, ICP-MS method, and atomic absorption method.
  • the yttrium oxyfluoride of the present invention may be in the form of powder, granule, bulk, film, dense or porous It may be.
  • the bulk shape is a shape having a size capable of recognizing the outer shape with the naked eye. For example, at least one of the three dimensions of length, width, and thickness is 1 mm or more. Refers to the shape.
  • the bulk yttrium oxyfluoride may be, for example, a sintered body or a crystalline body.
  • the film shape refers to one having a thickness smaller than the length and width among the three dimensions of length, width and thickness, and having a thickness of 1 mm or less.
  • Bulk yttrium oxyfluoride can be suitably produced as a sintered body by, for example, a method for producing stabilized yttrium oxyfluoride described later.
  • the film-like yttrium oxyfluoride is obtained, for example, by pulverizing a sintered body or a fired product obtained by the method for producing stabilized yttrium oxyfluoride described later, and this powder material is obtained by thermal spraying, aerosol deposition.
  • a film can be formed by subjecting it to a film forming method such as a position method, a PVD (physical vapor deposition method), or an ion plating method.
  • the sintered body here refers to a bulk shape.
  • the fired product includes not only a sintered body but also a powder form. Examples of the thermal spraying method include flame spraying, high-speed flame spraying, explosion spraying, laser spraying, plasma spraying, and laser / plasma composite spraying.
  • powdery yttrium oxyfluoride and granulated yttrium oxyfluoride obtained by granulating this can form film-like yttrium oxyfluoride as described above by using these as raw materials.
  • yttrium oxyfluoride it is possible to obtain a durability improvement effect by suppressing the phase transition.
  • the yttrium oxyfluoride of the present invention has a shape having a large effect of strain based on volume change such as a bulk shape and / or a film shape, cracks due to the suppression of phase transition in the yttrium oxyfluoride of the present invention It is preferable because it can directly enjoy the effect of improving crack prevention, that is, durability.
  • the yttrium oxyfluoride of the present invention is made into a bulk form such as a sintered body, it can be suitably used as a component of a semiconductor manufacturing apparatus as a bulk body having high halogen-resistant plasma resistance and ensuring durability. preferable.
  • any of the first raw material powder and the second raw material powder described later can be suitably used as the raw material powder for producing stabilized yttrium oxyfluoride.
  • the crystal structure of the yttrium oxyfluoride powder represented by YOF in the first raw material powder and the second raw material powder includes rhombohedral crystals or tetragonal crystals, and rhombohedral crystals are preferable from the viewpoint of availability. .
  • the first raw material powder is a mixed powder containing calcium fluoride powder represented by CaF 2 and yttrium oxyfluoride powder represented by YOF.
  • the amount of calcium fluoride powder in the first raw material powder is such that the number of moles of CaF 2 is 100 moles of YOF in the yttrium oxyfluoride powder.
  • the amount is preferably 8 mol or more and 40 mol or less, more preferably 10 mol or more and 35 mol or less, and further preferably 15 mol or more and 30 mol or less.
  • the amount is more preferably 15 mol or more and 25 mol or less.
  • the first raw material powder may contain other components other than the calcium fluoride powder represented by CaF 2 and the yttrium oxyfluoride powder represented by YOF, but the stabilized oxyfluoride using this raw material powder.
  • the total content of the fluoride powder and the yttrium oxyfluoride powder in the first raw material powder is preferably 50% by mass or more, and 80% by mass More preferably, it is more preferably 90% by mass or more. The higher the ratio of the total content in the first raw material powder, the better.
  • the average particle diameter D 50 of the oxyfluoride yttrium powder represented by YOF is preferably 1 ⁇ m or more 20 ⁇ m or less, 2 [mu] m or more 10 ⁇ m The following is more preferable. Further, from the viewpoint of obtaining the effect of the present invention more reliably and ensuring the mixing uniformity, the average particle diameter D 50 of the calcium fluoride powder represented by CaF 2 is preferably 10 ⁇ m or more and 100 ⁇ m or less, and 20 ⁇ m. More preferably, it is 50 ⁇ m or less. Measurement of average particle diameter D 50 is measured from the pretreated by sonication. The measurement can be performed by a laser diffraction / scattering particle size distribution measurement method, and specifically, can be measured by a method described later.
  • the second raw material powder is a mixed powder comprising a calcium fluoride powder represented by CaF 2, yttrium fluoride powder represented by YF 3, and the yttrium oxide powder represented by Y 2 O 3 .
  • the content of the yttrium oxide powder represented by Y 2 O 3 in the second raw material powder is The number of moles of Y 2 O 3 in the powder is preferably from 95 moles to 105 moles, more preferably from 99 moles to 101 moles, with respect to 100 moles of YF 3 in the yttrium fluoride powder.
  • the amount of calcium fluoride powder in the second raw material powder is expressed by YF 3 in terms of the number of moles of CaF 2 in the powder.
  • the total number of moles of yttrium atoms contained in the yttrium fluoride powder and the yttrium oxide powder represented by Y 2 O 3 is preferably 8 mol or more and 40 mol or less, preferably 10 mol or more and 35 mol or less. It is more preferable that it is 15 mol or more and 30 mol or less, and it is still more preferable that it is 15 mol or more and 25 mol or less.
  • the second raw material powder contains other components than calcium fluoride powder represented by CaF 2 , yttrium fluoride powder represented by YF 3 , and yttrium oxide powder represented by Y 2 O 3.
  • the fluoride powder and the yttrium fluoride in the second raw material powder The total content of the powder and the yttrium oxide powder is preferably 50% by mass or more, more preferably 80% by mass or more, and further preferably 90% by mass or more. The higher the ratio of the total content in the second raw material powder, the better.
  • the average particle diameter D 50 of yttrium fluoride powder is preferably 1 ⁇ m or more 20 ⁇ m or less, is 3 ⁇ m or 10 ⁇ m or less It is more preferable.
  • the D 50 of the yttrium oxide powder is more preferably preferably at 1 ⁇ m or more 20 ⁇ m or less is 3 ⁇ m or 10 ⁇ m or less.
  • the preferable range of the average particle diameter D 50 of the calcium fluoride powder it includes the same range as the preferred range of the average particle diameter D 50 of calcium fluoride powder in the first raw material powder.
  • the measurement can be performed by a laser diffraction / scattering particle size distribution measurement method, and specifically, can be measured by a method described later.
  • these raw material powders for producing stabilized yttrium oxyfluoride according to the present invention are subjected to a firing step described later, whereby yttrium oxyfluoride represented by YOF stabilized with calcium fluoride represented by CaF 2. Can be suitably obtained.
  • the suitable manufacturing method of the stabilized yttrium oxyfluoride of this invention is demonstrated.
  • the method for producing the stabilized yttrium oxyfluoride of the present invention any of the first method and the second method described below can be used.
  • the first method includes a step of firing a molded body of a mixed powder containing calcium fluoride powder represented by CaF 2 and yttrium oxyfluoride powder represented by YOF in an inert atmosphere or vacuum. .
  • the above-described first raw material powder can be suitably used.
  • the matters described above also apply to the mixed powder for the first raw material powder.
  • a method for obtaining a molded body of a mixed powder for example, a die press method, a rubber press (hydrostatic pressure press) method, a sheet molding method, an extrusion molding method, a casting molding method, or the like can be used.
  • the obtained molded body is fired under an inert atmosphere or under vacuum. Nitrogen or argon can be used as the inert atmosphere.
  • the firing temperature is 800 ° C. or higher and 1700 ° C. or lower. By setting the firing temperature to 800 ° C. or higher, the fluoride can be reliably dissolved in yttrium oxyfluoride. Moreover, by setting the firing temperature to 1700 ° C. or lower, it is possible to suppress the decomposition or modification of the oxyfluoride or to suppress the occurrence of cracks in the sintered body.
  • the firing temperature is preferably 800 ° C. or higher and 1700 ° C. or lower, and more preferably 1000 ° C. or higher and 1600 ° C. or lower.
  • the firing time is preferably 2 hours or more and 24 hours or less, and more preferably 4 hours or more and 12 hours or less.
  • the firing may be firing under pressure or firing under no pressure.
  • specific pressurizing methods during firing include hot pressing, pulsed current pressing (SPS), hot isostatic pressing (HIP), and the like.
  • SPS pulsed current pressing
  • HIP hot isostatic pressing
  • the second method is a compact of a mixed powder containing calcium fluoride powder represented by CaF 2 , yttrium fluoride powder represented by YF 3 , and yttrium oxide powder represented by Y 2 O 3. Is baked to produce yttrium oxyfluoride represented by YOF from YF 3 and Y 2 O 3 , and then baked under an inert atmosphere or under vacuum.
  • the mixed powder the above-described second raw material powder can be suitably used. All the matters described above also apply to the mixed powder for the second raw material powder.
  • the obtained molded body is fired to produce yttrium oxyfluoride represented by YOF from YF 3 and Y 2 O 3 .
  • the firing atmosphere at this time may be any of an oxygen-containing atmosphere such as air, a vacuum, and an inert atmosphere.
  • the inert atmosphere the same inert atmosphere as described in the first method can be used.
  • a vacuum and an inert atmosphere are preferable from the viewpoint of being able to be carried out continuously with high-temperature firing in the next stage.
  • the firing temperature is preferably 800 ° C. or higher from the viewpoint of efficiently producing yttrium oxyfluoride.
  • the firing temperature is more preferably 820 ° C. or higher and 980 ° C. or lower, and particularly preferably 850 ° C. or higher and 950 ° C. or lower.
  • the firing time is preferably 0.5 hours or more and 4 hours or less, and more preferably 1 hour or more and 2 hours or less.
  • the firing may be firing under pressure or firing under no pressure.
  • the fired product obtained by the firing is fired in an inert atmosphere or in a vacuum.
  • the inert gas used for the inert atmosphere the same gas as described in the first method can be used.
  • the firing temperature is preferably 800 ° C. or higher and 1700 ° C. or lower.
  • the firing temperature is preferably 800 ° C. or higher and 1700 ° C. or lower, and more preferably 1000 ° C. or higher and 1600 ° C. or lower.
  • the firing time is preferably 2 hours or longer and 24 hours or shorter, and more preferably 4 hours or longer and 12 hours or shorter.
  • the firing may be firing under pressure or firing under no pressure.
  • a specific pressurization method at the time of firing includes the same method as the pressurization method described in the first method.
  • the stabilized yttrium oxyfluoride of the present invention which is a sintered body, can be suitably obtained by any of the first and second methods described above.
  • the bulk-stabilized yttrium oxyfluoride thus obtained is used as an inner wall material of constituent members of a semiconductor manufacturing apparatus such as a vacuum chamber in an etching apparatus and a sample table, chuck, focus ring, etching gas supply port in the chamber. It can be used suitably.
  • Stabilized yttrium oxyfluoride can be used for various plasma processing apparatuses and chemical plant components in addition to the components of semiconductor manufacturing equipment.
  • the powdered product obtained by pulverizing bulk stabilized yttrium oxyfluoride is preferably used as a raw material for the film stabilized yttrium oxyfluoride, and the obtained film stabilized yttrium oxyfluoride is It can be suitably used for coating applications of semiconductor manufacturing equipment, in particular, coating of the inner wall of a chamber in semiconductor manufacturing equipment such as an etching apparatus.
  • Example 1 YOF powder (rhombohedral crystal, average particle diameter D 50 2.8 ⁇ m) and CaF 2 powder (average particle diameter D 50 33.5 ⁇ m) in an amount of 10 mol with respect to 100 moles of this YOF powder were mixed. A mixed powder was obtained. This mixed powder was put into a mold. The mold was circular in plan view, and the dimension was 25 mm. Using a hydraulic press as a molding method, a compact was obtained by uniaxially pressing at a pressure of 65 MPa for 0.5 minutes. The obtained molded body was fired at 1400 ° C. for 4 hours in an Ar atmosphere. This obtained the sintered compact which is stabilized yttrium oxyfluoride.
  • the average particle diameter is measured by the following method (the same applies hereinafter).
  • ⁇ Measurement method of average particle diameter D 50> Measurement was performed with a Microtrac HRA manufactured by Nikkiso Co., Ltd. At the time of measurement, a 2% sodium hexametaphosphate aqueous solution was used as a dispersion medium, and a slurry sample was added to the chamber of the microtrac HRA sample circulator until the apparatus determined that the concentration was appropriate. In this slurry sample, 1 g of powder was added to 100 ml of 0.2% sodium hexametaphosphate aqueous solution in a beaker, and this was set in an ultrasonic homogenizer (output 25 W) manufactured by Nikkiso Co., Ltd. for 2 minutes. It was prepared by performing.
  • the obtained sintered body was subjected to the following DTA measurement and TMA measurement.
  • DTA measurement was performed by raising the temperature from 25 ° C to 1000 ° C.
  • TMA measurement was performed by reciprocating the temperature from 25 ° C. to 1000 ° C. and the temperature decreasing from 1000 ° C. to 25 ° C.
  • a phase change of which a discontinuity point was confirmed was designated as “present”, and a phase transition which was not confirmed was designated as “no”.
  • the results are shown in Table 1.
  • Measurement apparatus DTG-60H (manufacturer: Shimadzu Corporation), atmosphere: Air, temperature program: measurement range; 25 ° C. to 1000 ° C., temperature increase rate: 5 ° C./min, reference: component alumina.
  • the sample amount was 60 mg.
  • ⁇ XRD measurement method Part of the sintered body was pulverized using a mortar and pestle to obtain a powder, and XRD measurement was performed on this powder.
  • Device name: MiniFlex600, manufacturer: Rigaku was used as a measuring instrument.
  • Examples 2 to 7, Comparative Example 4 A sintered body was produced in the same manner as in Example 1 except that the amount of CaF 2 powder was changed to the amount shown in Table 1 below with respect to 100 moles of YOF powder, and this was evaluated. The results are shown in Table 1.
  • the DTA chart obtained by DTA measurement is shown in FIG. 1
  • the TMA chart obtained by TMA measurement is shown in FIG. 2
  • the XRD chart obtained by XRD measurement is shown in FIG. Show.
  • the TEMP curve described with the thin continuous line in FIG. 2 has shown the sample temperature in each time in TMA measurement with the scale on the right side.
  • Example 1 A sintered body was produced in the same manner as in Example 1 except that LiF powder was used in the amount shown in Table 1 below with respect to 100 moles of YOF powder instead of CaF 2 powder, and this was evaluated. The results are shown in Table 1.
  • the charts obtained by performing the same DTA measurement, TMA measurement, and XRD measurement as those of Example 1 for the sintered body obtained in Comparative Example 1 are shown in FIGS. 4 to 6, respectively.
  • the thick line in FIG. 5 is a TMA chart obtained by TMA measurement
  • the TEMP curve described by a thin solid line shows the sample temperature at each time in TMA measurement on the right scale. ing.
  • Example 3 A sintered body was produced in the same manner as in Example 1 except that YF 3 powder was used in an amount shown in Table 1 below with respect to the number of moles of YOF powder of 100 instead of CaF 2 powder, and this was evaluated. . The results are shown in Table 1. In Table 1 below, “-” represents not implemented.
  • the sintered body of yttrium oxyfluoride obtained in each example was cubic at 25 ° C., and the X-ray diffraction peak derived from the rhombohedral crystal of yttrium oxyfluoride X-ray diffraction peaks derived from CaF 2 were not observed.
  • the yttrium oxyfluoride of each example stabilized with calcium fluoride is effective in the phase transition from cubic to rhombohedral when cooled from high temperature to room temperature. It can be seen that it is suppressed. In such a sintered body of yttrium oxyfluoride, cracks and cracks resulting from this phase transition are effectively prevented.
  • YF 3 powder (average particle diameter D 50 5.7 ⁇ m), Y 2 O 3 powder (average particle diameter D 50 3.1 ⁇ m) in the number of moles shown in Table 2 with respect to 100 moles of this YF 3 powder, Total number of moles of YF 3 powder and Y 2 O 3 powder (total number of moles of yttrium fluoride powder represented by YF 3 and number of moles of yttrium atoms contained in yttrium oxide powder represented by Y 2 O 3 ) 100 and the number of moles of CaF 2 powder (average particle size D 50 33.5 ⁇ m) shown in Table 2 was mixed to obtain a mixed powder.
  • a molded body was obtained from this mixed powder in the same manner as in Example 1.
  • the obtained molded body was fired at 900 ° C. for 2 hours in an Ar atmosphere. Subsequently, the fired body was fired at 1400 ° C. for 4 hours in an Ar atmosphere.
  • the two-stage firing was performed continuously in one firing batch.
  • a sintered body was obtained as described above. The obtained sintered body was subjected to the same evaluation as in Example 1. The results are shown in Table 2.

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Abstract

La présente invention concerne un oxyfluorure d'yttrium représenté par YOF et stabilisé par un fluorure représenté par CaF2. Le nombre de moles de Ca est de préférence de 8 moles à 40 moles (inclus) par rapport à 100 moles d'yttrium. Une poudre de matériau de départ selon la présente invention est composée d'une première poudre mixte contenant une poudre de fluorure de calcium représenté par CaF2 et une poudre d'oxyfluorure d'yttrium représenté par YOF, ou est composée, en variante, d'une seconde poudre mixte contenant une poudre de fluorure de calcium représenté par CaF2, une poudre de fluorure d'yttrium représenté par YF3 et une poudre d'oxyde d'yttrium représenté par Y2O3. Dans un procédé de production selon la présente invention, un corps moulé à partir de la première ou de la seconde poudre mixte est cuit dans des conditions prédéterminées.
PCT/JP2016/060240 2015-09-07 2016-03-29 Oxyfluorure d'yttrium, poudre de matériau de départ pour la production d'oxyfluorure d'yttrium stabilisé, et procédé de production d'oxyfluorure d'yttrium stabilisé WO2017043117A1 (fr)

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CN201680045497.6A CN107848831A (zh) 2015-09-07 2016-03-29 氟氧化钇、稳定化氟氧化钇制造用原料粉末以及稳定化氟氧化钇的制造方法
US15/749,432 US10280091B2 (en) 2015-09-07 2016-03-29 Yttrium oxyfluoride, starting material powder for production of stabilized yttrium oxyfluoride, and method for producing stabilized yttrium oxyfluoride
JP2017502743A JP6189570B2 (ja) 2015-09-07 2016-03-29 オキシフッ化イットリウム、安定化オキシフッ化イットリウム製造用原料粉末及び安定化オキシフッ化イットリウムの製造方法

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US10563303B2 (en) * 2017-05-10 2020-02-18 Applied Materials, Inc. Metal oxy-flouride films based on oxidation of metal flourides
KR20240032700A (ko) 2022-08-30 2024-03-12 주식회사 히타치하이테크 플라스마 처리 장치, 플라스마 처리 장치의 내부 부재, 및 플라스마 처리 장치의 내부 부재의 제조 방법

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WO2019132550A1 (fr) * 2017-12-29 2019-07-04 아이원스 주식회사 Procédé de formation d'un film de revêtement et film de revêtement formé par ce biais
JP7147675B2 (ja) * 2018-05-18 2022-10-05 信越化学工業株式会社 溶射材料、及び溶射部材の製造方法
KR102091744B1 (ko) * 2018-08-09 2020-03-20 (주)석경에이티 균일한 입자직경을 가지는 박막 코팅용 이트륨 옥시플루오라이드 또는 이트륨 플루오라이드 분말 및 그들의 제조방법

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KR20240032700A (ko) 2022-08-30 2024-03-12 주식회사 히타치하이테크 플라스마 처리 장치, 플라스마 처리 장치의 내부 부재, 및 플라스마 처리 장치의 내부 부재의 제조 방법

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